EP1776442B1 - A highly water-soluble solid laundry detergent composition that forms a clear wash liquor upon dissolution in water - Google Patents
A highly water-soluble solid laundry detergent composition that forms a clear wash liquor upon dissolution in water Download PDFInfo
- Publication number
- EP1776442B1 EP1776442B1 EP05786488A EP05786488A EP1776442B1 EP 1776442 B1 EP1776442 B1 EP 1776442B1 EP 05786488 A EP05786488 A EP 05786488A EP 05786488 A EP05786488 A EP 05786488A EP 1776442 B1 EP1776442 B1 EP 1776442B1
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- EP
- European Patent Office
- Prior art keywords
- composition
- surfactant
- composition according
- detersive surfactant
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- Prior art date
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- 239000000203 mixture Substances 0.000 title claims description 234
- 239000003599 detergent Substances 0.000 title claims description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 26
- 239000007787 solid Substances 0.000 title claims description 15
- 238000004090 dissolution Methods 0.000 title description 17
- 239000004094 surface-active agent Substances 0.000 claims description 267
- 125000000129 anionic group Chemical group 0.000 claims description 120
- -1 alkylbenzene sulphonate Chemical class 0.000 claims description 69
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 62
- 125000002091 cationic group Chemical group 0.000 claims description 44
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 44
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 31
- 229910021536 Zeolite Inorganic materials 0.000 claims description 28
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 28
- 239000010457 zeolite Substances 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 26
- 150000003839 salts Chemical class 0.000 claims description 21
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 20
- 239000002689 soil Substances 0.000 claims description 18
- 229910019142 PO4 Inorganic materials 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 17
- 239000010452 phosphate Substances 0.000 claims description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 16
- 150000004760 silicates Chemical class 0.000 claims description 15
- 239000007844 bleaching agent Substances 0.000 claims description 12
- 125000000963 oxybis(methylene) group Chemical group [H]C([H])(*)OC([H])([H])* 0.000 claims description 12
- 238000004806 packaging method and process Methods 0.000 claims description 11
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 238000007046 ethoxylation reaction Methods 0.000 claims description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 229920005646 polycarboxylate Polymers 0.000 claims description 7
- 238000012546 transfer Methods 0.000 claims description 7
- 108091005804 Peptidases Proteins 0.000 claims description 6
- 239000004365 Protease Substances 0.000 claims description 6
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 5
- ZXGOACRTCPRVON-UHFFFAOYSA-K trisodium;2-sulfonatobutanedioate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(C([O-])=O)S([O-])(=O)=O ZXGOACRTCPRVON-UHFFFAOYSA-K 0.000 claims description 3
- 230000002087 whitening effect Effects 0.000 claims description 2
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 claims 2
- 239000002245 particle Substances 0.000 description 54
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 37
- 150000005323 carbonate salts Chemical class 0.000 description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 21
- 238000004140 cleaning Methods 0.000 description 20
- 229910052938 sodium sulfate Inorganic materials 0.000 description 19
- 235000011152 sodium sulphate Nutrition 0.000 description 18
- 229910052791 calcium Inorganic materials 0.000 description 13
- 239000011575 calcium Substances 0.000 description 13
- 239000004744 fabric Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 125000004066 1-hydroxyethyl group Chemical group [H]OC([H])([*])C([H])([H])[H] 0.000 description 10
- 150000004996 alkyl benzenes Chemical class 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 9
- 125000000217 alkyl group Chemical group 0.000 description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 8
- 150000001768 cations Chemical class 0.000 description 8
- 229920001577 copolymer Polymers 0.000 description 8
- 239000012876 carrier material Substances 0.000 description 7
- 239000003093 cationic surfactant Substances 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 5
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 5
- 238000004900 laundering Methods 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 238000012423 maintenance Methods 0.000 description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 5
- 239000011976 maleic acid Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Natural products OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 239000012190 activator Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 239000002736 nonionic surfactant Substances 0.000 description 4
- 239000002304 perfume Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- VKZRWSNIWNFCIQ-WDSKDSINSA-N (2s)-2-[2-[[(1s)-1,2-dicarboxyethyl]amino]ethylamino]butanedioic acid Chemical compound OC(=O)C[C@@H](C(O)=O)NCCN[C@H](C(O)=O)CC(O)=O VKZRWSNIWNFCIQ-WDSKDSINSA-N 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 3
- 108010065511 Amylases Proteins 0.000 description 3
- 102000013142 Amylases Human genes 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- 108090001060 Lipase Proteins 0.000 description 3
- 239000004367 Lipase Substances 0.000 description 3
- 102000004882 Lipase Human genes 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- BGRWYDHXPHLNKA-UHFFFAOYSA-N Tetraacetylethylenediamine Chemical compound CC(=O)N(C(C)=O)CCN(C(C)=O)C(C)=O BGRWYDHXPHLNKA-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 3
- 235000019418 amylase Nutrition 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 230000000536 complexating effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 235000019421 lipase Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- 235000019341 magnesium sulphate Nutrition 0.000 description 3
- 239000001630 malic acid Substances 0.000 description 3
- 235000011090 malic acid Nutrition 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 235000012149 noodles Nutrition 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000015227 regulation of liquid surface tension Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000001384 succinic acid Substances 0.000 description 3
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical class NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 description 3
- 239000004382 Amylase Substances 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
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- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
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- 239000000460 chlorine Substances 0.000 description 2
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- 230000037431 insertion Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- YZVJHCGMTYDKFR-UHFFFAOYSA-L magnesium;disulfamate Chemical compound [Mg+2].NS([O-])(=O)=O.NS([O-])(=O)=O YZVJHCGMTYDKFR-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 108010087558 pectate lyase Proteins 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-K pentetate(3-) Chemical compound OC(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O QPCDCPDFJACHGM-UHFFFAOYSA-K 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- UHGWBEXBBNLGCZ-UHFFFAOYSA-N phenyl nonanoate Chemical compound CCCCCCCCC(=O)OC1=CC=CC=C1 UHGWBEXBBNLGCZ-UHFFFAOYSA-N 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 229920000075 poly(4-vinylpyridine) Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- YDJJYISOOCYHQU-UHFFFAOYSA-L zinc;disulfamate Chemical compound [Zn+2].NS([O-])(=O)=O.NS([O-])(=O)=O YDJJYISOOCYHQU-UHFFFAOYSA-L 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/37—Mixtures of compounds all of which are anionic
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/65—Mixtures of anionic with cationic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/86—Mixtures of anionic, cationic, and non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
Definitions
- the present invention relates to a highly water-soluble solid laundry detergent composition that upon dissolution in water forms a clear wash liquor. More specifically, the present invention relates to a solid laundry detergent composition comprising an anionic detersive surfactant system and low or no levels of zeolite builder, phosphate builder and silicate salt.
- Granular laundry detergent compositions need to have a very good fabric-cleaning performance against a wide variety of soil types.
- Granular laundry detergents also need to have very good dispensing and dissolution profiles.
- a dichotomy may exist in that some reformulations of the granular laundry detergent composition to improve its fabric-cleaning performance may negatively impact its dispensing and dissolution profiles, and vice versa. It is very difficult to improve the cleaning performance, dispensing profile and dissolution profile of a granular laundry detergent composition at the same time.
- Anionic detersive surfactants are incorporated into granular laundry detergent compositions in order to provide a good fabric-cleaning benefit.
- GB 1408969 , GB 1408970 , US4487710 , US5663136 and WO2004/041982 all relate to compositions comprising anionic detersive surfactants.
- the anionic detersive surfactant is capable of complexing with free cations, such as calcium and magnesium cations, that are present in the wash liquor in such a manner as to cause the anionic detersive surfactant to precipitate out of solution, which leads to a reduction in the anionic detersive surfactant activity.
- these water-insoluble complexes may deposit onto the fabric resulting in poor whiteness maintenance and poor fabric integrity benefits. This is especially problematic when the laundry detergent composition is used in hard-water washing conditions when there is a high concentration of calcium cations.
- zeolite builders which have a high binding constant with cations such as calcium and magnesium cations.
- cations such as calcium and magnesium cations.
- zeolite builders are water-insoluble and their incorporation in laundry detergent compositions leads to poor dissolution of the laundry detergent composition and can also lead to undesirable residues being deposited on the fabric.
- detergent compositions that comprise high levels of zeolite builder form undesirable cloudy wash liquors upon contact with water.
- phosphate builders allegedly do not have favourable environmental profiles and their use in laundry detergent compositions is becoming less common; for example, due to phosphate legislation in many countries.
- Detergent compositions comprising alkyl benzene sulphonate and alkyl ethoxylated sulphate detersive surfactants are described in GB 1408969 , GB 1408970 , US4487710 and US5663136 .
- a detergent composition comprising an anionic detersive surfactant and a non-ionic detersive surfactant that allegedly gives enhanced stain removal at a wide range of water-hardness is described in WO2004/041982 .
- a combination of a granular detergent and a packaging system having a low moisture vapour transfer rate is described in EP634484 .
- a granular laundry detergent composition comprising an anionic detersive surfactant having a good fabric-cleaning performance, especially a good greasy stain cleaning performance, good whiteness maintenance, and very good dispensing and dissolution profiles, and which upon dissolution in water gives a clear wash liquor.
- the present invention provides a solid laundry detergent composition as defined in claim 1.
- the composition comprises from 0.1wt% to 10wt% of an alkoxylated anionic detersive surfactant. This is the optimal level of alkoxylated anionic detersive surfactant to provide good greasy soil cleaning performance, to give a good sudsing profile, and to improve the hardness tolerancy of the overall detersive surfactant system. It may be preferred for the composition to comprise from 3wt% to 5wt% alkoxylated anionic detersive surfactant, or it may be preferred for the composition to comprise from 1wit% to 3wt% alkoxylated anionic detersive surfactant.
- the alkoxylated anionic detersive surfactant is a linear or branched, substituted or unsubstituted C 12-18 alkyl alkoxylated sulphate having an average degree of alkoxylation of from 1 to 30, preferably from 1 to 10.
- the alkoxylated anionic detersive surfactant is a linear or branched, substituted or unsubstituted C 12-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 1 to 10.
- the alkoxylated anionic detersive surfactant is a linear unsubstituted C 12-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 3 to 7.
- the alkoxylated anionic detersive surfactant is in the form of a non-spray-dried powder such as an extrudate, agglomerate, preferably an agglomerate. This is especially preferred when it is desirable to incorporate high levels of alkoxylated anionic detersive surfactant in the composition.
- the alkoxylated anionic detersive surfactant may also increase the non-alkoxylated anionic detersive surfactant activity by making the non-alkoxylated anionic detersive surfactant less likely to precipitate out of solution in the presence of free calcium cations.
- the weight ratio of non-alkoxylated anionic detersive surfactant to alkoxylated anionic detersive surfactant is less than 5:1, or less than 3:1, or less than 1.7:1, or even less than 1.5:1. This ratio gives optimal whiteness maintenance performance combined with a good hardness tolerency profile and a good sudsing profile.
- the weight ratio of non-alkoxylated anionic detersive surfactant to alkoxylated anionic detersive surfactant is greater than 5:1, or greater than 6:1, or greater than 7:1, or even greater than 10:1. This ratio gives optimal greasy soil cleaning performance combined with a good hardness tolerency profile, and a good sudsing profile.
- Suitable alkoxylated anionic detersive surfactants are: Texapan LEST TM by Cognis; Cosmacol AES TM by Sasol; BES151 TM by Stephan; Empicol ESC70/U TM ; and mixtures thereof.
- the composition comprises from 1 wt% to 25wt% of a non-alkoxylated anionic detersive surfactant. This is the optimal level of non-alkoxylated anionic detersive surfactant to provide a good cleaning performance. It may be preferred for the composition to comprise from 16wt% to 20wt% of a non-alkoxylated alkoxylated anionic detersive surfactant. This is especially preferred when the composition comprises from 1wt% to 3wt% alkoxylated anionic detersive surfactant. These amounts of anionic detersive surfactant provide a good greasy cleaning performance combined with a good hardness tolerency profile and a good sudsing profile.
- composition may also be preferred for the composition to comprise from 4wt% to 10wt% non-alkoxylated anionic detersive surfactant. This is especially preferred when the composition comprises from 3wt% to 5wt% alkoxylated anionic detersive surfactant. These amounts of anionic detersive surfactant provide a good whiteness maintenance profile combined with a good hardness tolerency profile and a good sudsing profile.
- the non-alkoxylated anionic detersive surfactant can be an alkyl sulphate, an alkyl sulphonate, an alkyl phosphate, an alkyl phosphonate, an alkyl carboxylate or any mixture thereof.
- the non-alkoxylated anionic surfactant can be selected from the group consisting of: C 10 -C 18 alkyl benzene sulphonates (LAS) preferably C 10 -C 13 alkyl benzene sulphonates; C 10 -C 20 primary, branched-chain, linear-chain and random-chain alkyl sulphates (AS), typically having the following formula: CH 3 (CH 2 ) x CH 2 -OSO 3 - M + wherein, M is hydrogen or a cation which provides charge neutrality, preferred cations are sodium and ammonium cations, wherein x is an integer of at least 7, preferably at least 9; C 10 -C 18 secondary (2,3) alkyl sulphates, typically having the following formulae: wherein, M is hydrogen or a cation which provides charge neutrality, preferred cations include sodium and ammonium cations, wherein x is an integer of at least 7, preferably at least 9, y is an integer of at least 8,
- Preferred non-alkoxylated anionic detersive surfactants are selected from the group consisting of: linear or branched, substituted or unsubstituted, C 12-18 alkyl sulphates; linear or branched, substituted or unsubstituted, C 10-13 alkylbenzene sulphonates, preferably linear C 10-13 alkylbenzene sulphonates; and mixtures thereof. Highly preferred are linear C 10-13 alkylbenzene sulphonates.
- linear C 10-13 alkylbenzene sulphonates that are obtainable, preferably obtained, by sulphonating commercially available linear alkyl benzenes (LAB);
- suitable LAB include low 2-phenyl LAB, such as those supplied by Sasol under the tradename Isochem ® or those supplied by Petresa under the tradename Petrelab ® , other suitable LAB include high 2-phenyl LAB, such as those supplied by Sasol under the tradename Hyblene ® .
- non-alkoxylated anionic detersive surfactant may be structurally modified in such a manner as to cause the non-alkoxylated anionic detersive surfactant to be more calcium tolerant and less likely to precipitate out of the wash liquor in the presence of free calcium ions.
- This structural modification could be the introduction of a methyl or ethyl moiety in the vicinity of the non-alkoxylated anionic detersive surfactant's head group, as this can lead to a more calcium tolerant non-alkoxylated anionic detersive surfactant due to steric hindrance of the head group, which may reduce the non-alkoxylated anionic detersive surfactant's affinity for complexing with free calcium cations in such a manner as to cause precipitation out of solution.
- the non-alkoxylated anionic detersive surfactant is in particulate form, such as an agglomerate, a spray-dried powder, an extrudate, a bead, a noodle, a needle or a flake.
- the non-alkoxylated anionic detersive surfactant, or at least part thereof is in agglomerate form; the agglomerate preferably comprising at least 20%, by weight of the agglomerate, of a non-alkoxylated anionic detersive surfactant, more preferably from 25wt% to 65wt%, by weight of the agglomerate, of a non-alkoxylated anionic detersive surfactant.
- part of the non-alkoxylated anionic detersive surfactant may be in the form of a spray-dried powder (e.g. a blown powder), and for part of the non-alkoxylated anionic detersive surfactant to be in the form of a non-spray-dried powder (e.g. an agglomerate, or an extrudate, or a flake such as a linear alkyl benzene sulphonate flake; suitable linear alkyl benzene sulphonate flakes are supplied by Pilot Chemical under the tradename F90 ® , or by Stepan under the tradename Nacconol 90G ® ). This is especially preferred when it is desirable to incorporate high levels of non-alkoxylated anionic detersive surfactant in the composition.
- a spray-dried powder e.g. a blown powder
- part of the non-alkoxylated anionic detersive surfactant may be in the form of a non-s
- the composition optionally may comprise from 0.1 wt% to 5wt% cationic detersive surfactant.
- the composition comprises from 0.5wt% to 3wt%, or from 1% to 3wt%, or even from 1 wt% to 2wt% cationic detersive surfactant. This is the optimal level of cationic detersive surfactant to provide good cleaning.
- Suitable cationic detersive surfactants are alkyl pyridinium compounds, alkyl quaternary ammonium compounds, alkyl quaternary phosphonium compounds, and alkyl ternary sulphonium compounds.
- the cationic detersive surfactant can be selected from the group consisting of: alkoxylate quaternary ammonium (AQA) surfactants as described in more detail in US 6,136,769 ; dimethyl hydroxyethyl quaternary ammonium as described in more detail in US 6,004,922 ; polyamine cationic surfactants as described in more detail in WO 98/35002 , WO 98/35003 , WO 98/35004 , WO 98/35005 , and WO 98/35006 ; cationic ester surfactants as described in more detail in US 4,228,042 , US 4,239,660 , US 4,260,529 and US 6,022,844 ; amino surfactants as described in more detail in US 6,221,825 and WO 00/47708 , specifically amido propyldimethyl amine; and mixtures thereof.
- AQA alkoxylate quaternary ammonium
- Preferred cationic detersive surfactants are quaternary ammonium compounds having the general formula: (R)(R 1 )(R 2 )(R 3 )N + X - wherein, R is a linear or branched, substituted or unsubstituted C 6-18 alkyl or alkenyl moiety, R 1 and R 2 are independently selected from methyl or ethyl moieties, R 3 is a hydroxyl, hydroxymethyl or a hydroxyethyl moiety, X is an anion which provides charge neutrality, preferred anions include halides (such as chloride), sulphate and sulphonate.
- Preferred cationic detersive surfactants are mono-C 6-18 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chlorides. Highly preferred cationic detersive surfactants are mono-C 8-10 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride, mono-C 10-12 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride and mono-C 10 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride.
- the cationic detersive surfactant provides additional greasy soil cleaning performance.
- the cationic detersive surfactant may increase the tendency of the non-alkoxylated anionic detersive surfactant to precipitate out of solution.
- the cationic detersive surfactant and the non-alkoxylated anionic detersive surfactant are present in the composition in the form of separate particles. This minimises any effect that the cationic detersive surfactant may have on the undesirable precipitation of the non-alkoxylated anionic detersive surfactant, and also ensures that upon contact with water, the resultant wash liquor is not cloudy.
- the weight ratio of non-alkoxylated anionic detersive surfactant to cationic detersive surfactant is in the range of from 5:1 to 25:1, more preferably from 5:1 to 20:1 or from 6:1 to 15:1, or from 7:1 to 10:1, or even from 8:1 1 to 9:1.
- the cationic detersive surfactant is preferably in particulate form, such as a spray-dried powder, an agglomerate, an extrudate, a flake, a noodle, a needle, or any combination thereof.
- the cationic detersive surfactant, or at least part thereof is in the form of a spray-dried powder or an agglomerate.
- the composition may comprises from 0.5wt% to 10wt% non-ionic detersive surfactant.
- the composition may comprises from 1wt% to 7wt% or from 2wt% to 4wt% non-ionic detersive surfactant.
- the inclusion of non-ionic detersive surfactant in the composition helps to provide a good overall cleaning profile, especially when laundering at high temperatures such as 60°C or higher.
- the non-ionic detersive surfactant could be an alkyl polyglucoside and/or an alkyl alkoxylated alcohol.
- the non-ionic detersive surfactant is a linear or branched, substituted or unsubstituted C 8-18 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 10, more preferably from 3 to 7.
- the non-ionic detersive surfactant not only provides additional greasy soil cleaning performance but may also increase the anionic detersive surfactant activity by making the anionic detersive surfactant less likely to precipitate out of solution in the presence of free calcium cations.
- the weight ratio of non-alkoxylated anionic detersive surfactant to non-ionic detersive surfactant is in the range of less than 8:1, or less than 7:1, or less than 6:1 or less than 5:1, preferably from 1:1 to 5:1, or from 2:1 to 5:1, or even from 3:1 to 4:1.
- the non-ionic detersive surfactant, or at least part thereof can be incorporated into the composition in the form of a liquid spray-on, wherein the non-ionic detersive surfactant, or at least part thereof, in liquid form (e.g. in the form of a hot-melt) is sprayed onto the remainder of the composition.
- the non-ionic detersive surfactant, or at least part thereof may be in particulate form, and the non-ionic detersive surfactant, or at least part thereof, may be dry-added to the remainder of the composition.
- the non-ionic surfactant, or at least part thereof may be in the form of a co-particulate admixture with a solid carrier material such as carbonate salt, sulphate salt, burkeite, silica or any mixture thereof.
- the non-ionic detersive surfactant may be in a co-particulate admixture with either an alkoxylated anionic detersive surfactant, a non-alkoxylated anionic detersive surfactant or a cationic detersive surfactant.
- the non-ionic detersive surfactant, or at least part thereof may be agglomerated or extruded with either an alkoxylated anionic detersive surfactant, a non-alkoxylated anionic detersive surfactant or a cationic detersive surfactant.
- the composition comprises at least two separate surfactant components, each in particulate form. It may be preferred for the composition to comprise at least three separate surfactant components, each in particulate form.
- the first surfactant component predominantly comprises an alkoxylated detersive surfactant.
- predominantly comprises it is meant that the first surfactant component comprises greater than 50%, by weight of the first surfactant component, of an alkoxylated anionic detersive surfactant, preferably greater than 60%, or greater than 70%, or greater than 80%, or greater than 90% or even essentially 100%, by weight of the first surfactant component, of an alkoxylated anionic detersive surfactant.
- the first surfactant component comprises less than 10%, by weight of the first surfactant component, of a non-alkoxylated anionic detersive surfactant, preferably less than 5%, or less than 2%, or even 0%, by weight of the first surfactant component, of a non-alkoxylated anionic detersive surfactant.
- the first surfactant component is essentially free from non-alkoxylated anionic detersive surfactant.
- essentially free from non-alkoxylated anionic detersive surfactant it is typically meant that the first surfactant component comprises no deliberately added non-alkoxylated anionic detersive surfactant. This is especially preferred in order to ensure that the composition has good dispensing and dissolution profiles, and also to ensure that the composition provides a clear wash liquor upon dissolution in water.
- the first surfactant component comprises less than 10%, by weight of the first surfactant component, of a cationic detersive surfactant, preferably less than 5%, or less than 2%, or even 0%, by weight of the first surfactant component, of a cationic detersive surfactant.
- the first surfactant component is essentially free from cationic detersive surfactant.
- essentially free from cationic detersive surfactant it is typically meant that the first surfactant component comprises no deliberately added cationic detersive surfactant. This is especially preferred in order to reduce the degree of surfactant gelling in the wash liquor.
- the first surfactant component is preferably in the form of a spray-dried powder, an agglomerate, an extrudate or a flake. If the first surfactant component is in the form of an agglomerate particle or an extrudate particle, then preferably the particle comprises from 20% to 65%, by weight of the particle, of an alkoxylated anionic detersive surfactant. If the first surfactant component is in spray-dried particle form, then preferably the particle comprises from 10wt% to 30wt%, by weight of the particle, of an alkoxylated anionic detersive surfactant.
- the first surfactant component may be in the form of a co-particulate admixture with a solid carrier material.
- the solid carrier material can be a sulphate salt and/or a carbonate salt, preferably sodium sulphate and/or sodium carbonate.
- the second surfactant component predominantly comprises a non-alkoxylated detersive surfactant.
- the second surfactant component comprises greater than 50%, by weight of the second surfactant component, of a non-alkoxylated anionic detersive surfactant, preferably greater than 60%, or greater than 70%, or greater than 80%, or greater than 90% or even essentially 100%, by weight of the second surfactant component, of a non-alkoxylated anionic detersive surfactant.
- the second surfactant component comprises less than 10%, by weight of the second surfactant component, of an alkoxylated anionic detersive surfactant, preferably less than 5%, or less than 2%, or even 0%, by weight of the second surfactant component, of an alkoxylated anionic detersive surfactant.
- the second surfactant component comprises less than 10%, by weight of the second surfactant component, of a cationic detersive surfactant, preferably less than 5%, or less than 2%, or even 0%, by weight of the second surfactant component, of a cationic detersive surfactant.
- the second surfactant component is essentially free from alkoxylated anionic detersive surfactant.
- alkoxylated anionic detersive surfactant it is typically meant that the second surfactant component comprises no deliberately added alkoxylated anionic detersive surfactant.
- the second surfactant component is essentially free from cationic detersive surfactant.
- essentially free from cationic detersive surfactant it is typically meant that the second surfactant component comprises no deliberately added cationic detersive surfactant. This is especially preferred in order to ensure that the composition has good dispensing and dissolution profiles, and also to ensure that the composition provides a clear wash liquor upon dissolution in water.
- the second surfactant component is preferably in the form of a spray-dried powder, a flash-dried powder, an agglomerate or an extrudate. If the second surfactant component is in the form of an agglomerate particle, then preferably the particle from 5% to 50%, by weight of the particle, of a non-alkoxylated anionic detersive surfactant, or from 5wt% to 25wt% non-alkoxylated anionic detersive surfactant.
- the second surfactant component may be in form of a co-particulate admixture with a solid carrier material.
- the solid carrier material can be a sulphate salt and/or a carbonate salt, preferably sodium sulphate and/or sodium carbonate.
- the third surfactant component predominantly comprises a cationic detersive surfactant.
- the third surfactant component comprises greater than 50%, by weight of the third surfactant component, of a cationic detersive surfactant, preferably greater than 60%, or greater than 70%, or greater than 80%, or greater than 90% or even essentially 100%, by weight of the third surfactant component, of a cationic detersive surfactant.
- the third surfactant component comprises less than 10%, by weight of the third surfactant component, of an alkoxylated anionic detersive surfactant, preferably less than 5%, or less than 2%, or even essentially 0%, by weight of the third surfactant component, of an alkoxylated anionic detersive surfactant.
- the third surfactant component comprises less than 10%, by weight of the third surfactant component, of a non-alkoxylated anionic detersive surfactant, preferably less than 5%, or less than 2%, or even 0%, by weight of the third surfactant component, of a non-alkoxylated anionic detersive surfactant.
- the third surfactant component is essentially free from alkoxylated anionic detersive surfactant.
- alkoxylated anionic detersive surfactant it is typically meant that the third surfactant component comprises no deliberately added alkoxylated anionic detersive surfactant.
- the third surfactant component is essentially free from non-alkoxylated anionic detersive surfactant.
- non-alkoxylated anionic detersive surfactant By essentially free from non-alkoxylated anionic detersive surfactant it is typically meant that the third surfactant component comprises no deliberately added non-alkoxylated anionic detersive surfactant. This is especially preferred in order to ensure that the composition has good dispensing and dissolution profiles, and also to ensure that the composition provides a clear wash liquor upon dissolution in water.
- the third surfactant component is preferably in the form of a spray-dried powder, a flash-dried powder, an agglomerate or an extrudate. If the third surfactant component is in the form of an agglomerate particle, then preferably the particle comprises from 5% to 50%, by weight of the particle, of cationic detersive surfactant, or from 5wt% to 25wt% cationic detersive surfactant.
- the third surfactant component may be in form of a co-particulate admixture with a solid carrier material.
- the solid carrier material can be a sulphate salt and/or a carbonate salt, preferably sodium sulphate and/or sodium carbonate.
- the detergent composition comprises from 0wt% to 10wt% silicate salt.
- the composition preferably comprises from 0wt% to 5wt%, or less than 4wt%, or less than 2wt%, or less than 1wt% silicate salt. It may even be preferred for the composition to be essentially free from silicate salt. By essentially free from silicate salt it is meant that the composition comprises no deliberately added silicate. This is especially preferred in order to ensure that the composition has a very good dispensing and dissolution profiles and to ensure that the composition provides a clear wash liquor upon dissolution in water.
- Silicate salts include water-insoluble silicates.
- Silicate salts include amorphous silicates and crystalline layered silicates (e.g. SKS-6).
- a preferred silicate salt is sodium silicate.
- the composition comprises from 0wt% to 4wt% zeolite builder.
- the composition preferably comprises from 0wt% to 3wt%, or from 0wt% to 2wt%, or from 0wt% to 1wt% zeolite builder. It may even be preferred for the composition to be essentially free from zeolite builder. By essentially free from zeolite builder it is typically meant that the composition comprises no deliberately added zeolite builder. This is especially preferred if it is desirable for the composition to be very highly soluble, to minimise the amount of water-insoluble residues (for example, which may deposit on fabric surfaces), and also when it is highly desirable to have transparent wash liquor.
- Zeolite builders include zeolite A, zeolite X, zeolite P and zeolite MAP.
- the composition comprises from 0wt% to 4wt% phosphate builder.
- the composition preferably comprises from 0wt% to 3wt%, or from 0wt% to 2wt%, or from 0wt% to 1wt% phosphate builder.
- By essentially free from phosphate builder it is typically meant that the composition comprises no deliberately added phosphate builder. This is especially preferred if it is desirable for the composition to have a very good environmental profile.
- Phosphate builders include sodium tripolyphosphate.
- composition may comprise adjunct builders other than the zeolite builder and phosphate builder, especially preferred are water-soluble adjunct builders.
- Adjunct builders are preferably selected from the group consisting of sodium carbonate, sulphamic acid and/or water-soluble salts thereof such as sodium sulphamate, citric acid and/or water soluble salts thereof such as sodium citrate; polymeric polycarboxylates such as co-polymers of acrylic acid and maleic acid, or polyacrylate.
- composition may comprise very low levels of water-insoluble builders such as zeolite A, zeolite X, zeolite P and zeolite MAP whilst comprising relatively high levels of water-soluble adjunct builders, such as sodium carbonate, sulphamic acid and citric acid. It may be preferred for the weight ratio of sodium carbonate to zeolite builder to be at least 5:1, preferably at least 10:1, or at least 15:1, or at least 20:1 or even at least 25:1.
- the detergent composition may comprise a carbonate salt, typically from 1wt% to 50wt%, or from 5wt% to 25wt% or from 10wt% to 20wt% carbonate salt.
- a preferred carbonate salt is sodium carbonate and/or sodium bicarbonate.
- a highly preferred carbonate salt is sodium carbonate.
- the composition may comprise from 10wt% to 20wt% sodium carbonate.
- the carbonate salt, or at least part thereof is typically in particulate form, typically having a weight average particle size in the range of from 200 to 500 micrometers. However, it may be preferred for the carbonate salt, or at least part thereof, to be in micronised particulate form, typically having a weight average particle size in the range of from 4 to 40 micrometers; this is especially preferred when the carbonate salt, or at least part thereof, is in the form of a co-particulate admixture with a detersive surfactant, such as an alkoxylated anionic detersive surfactant.
- a detersive surfactant such as an alkoxylated anionic detersive surfactant.
- High levels of carbonate improve the cleaning performance of the composition by increasing the pH of the wash liquor. This increased alkalinity improves the performance of the bleach, if present, increases the tendency of soils to hydrolyse which facilitates their removal from the fabric, and also increases the rate and degree of ionization of the soils to be cleaned; ionized soils are more soluble and easier to remove from the fabrics during the washing stage of the laundering process.
- high carbonate levels improve the flowability of the composition when the detergent composition is in free-flowing particulate form.
- the composition comprises low levels of, or no, carbonate salt.
- the composition may comprise from 0wt% to 10wt% carbonate salt to minimize the negatives associated with the presence of carbonate.
- it may be desirable to incorporate higher levels of carbonate salt in the composition.
- the composition also preferably comprises a source of acid that is capable of undergoing an acid/base reaction with a carbonate anion, such as sulphamic acid, citric acid, maleic acid, malic acid, succinic acid or any mixture thereof.
- a source of acid such as sulphamic acid, citric acid, maleic acid, malic acid, succinic acid or any mixture thereof.
- An especially preferred source of acid is sulphamic acid.
- the weight ratio of carbonate salt to the total amount of source of acid in the composition that is capable of undergoing an acid/base reaction with a carbonate anion is preferably less than 50:1, more preferably less than 25:1, or less than 15:1, or less than 10:1 or even less than 5:1.
- the composition comprises sodium carbonate and sulphamic acid, then preferably the weight ratio of sodium carbonate to sulphamic acid is less than 5:1.
- the total amount of carbonate anion source in the composition is preferably limited.
- Preferred carbonate anion sources are carbonate salts and/or percarbonate salts.
- the total amount of carbonate anion source (on a carbonate anion basis) in the composition is between 7wt% to 14wt% greater than the theoretical amount of carbonate anion source that is required to completely neutralise the total amount of acid source present in the composition that is capable of undergoing an acid/base reaction with a carbonate anion.
- the composition may preferably comprise at least 10wt% sulphate salt.
- High levels of sulphate salt can improve the greasy stain removal cleaning performance of the composition.
- a preferred sulphate salt is sodium sulphate.
- Sodium sulphate and sulphamic acid are capable of complexing together in the presence of water to form a complex having the formula: 6 HSO 3 NH 2 ⁇ 5 Na 2 SO 4 ⁇ 15 H 2 O Such complexes are suitable for use herein.
- the composition may preferably comprise very high levels of sulphate; the detergent composition typically comprises at least 15wt% sulphate salt, or even 20wt% sulphate salt, or even 25wt% sulphate salt and sometimes even at least 30wt% sulphate salt.
- the sulphate salt, or at least part thereof is typically in particulate form, typically having a weight average particle size in the range of from 60 to 200 micrometers. However, it may be preferred that the sulphate salt, or at least part thereof, is in micronised particulate form, typically having a weight average particle size in the range of from 5 to less than 60 micrometers, preferably from 5 to 40 micrometers.
- the sulphate salt may be in coarse particulate form, typically having a weight average particle size of from above 200 to 800 micrometers. However, it may also be preferred for the composition to comprise less than 20wt% sulphate salt, or even less than 10wt% or even less than 5wt% sulphate salt.
- the composition may preferably comprise less than 60wt% total combined amount of carbonate salt and sulphate salt.
- the composition may comprise less than 55wt%, or less than 50wt%, or less than 45wt%, or less than 40wt% total combined amount of carbonate salt and sulphate salt.
- the composition may comprise sulphamic acid and/or water-soluble salts thereof.
- the water-soluble salts of sulphamic acid can be alkali-metal or an alkaline-earth-metal salts of sulphamate.
- Other examples of water-soluble salts of sulphamic acid include ammonium sulphamate, zinc sulphamate and lead sulphamate.
- a preferred water-soluble salt of sulphamic acid is sodium sulphamate.
- the detergent composition comprises sulphamic acid.
- the detergent composition preferably comprises (on a sulphamic acid basis) from 0.1 wt% to 20wt% sulphamic acid, and/or water soluble salts thereof, however it may be preferred that the detergent composition comprises from 0.1wt% to 15wt%, or from 1wt% to 12wt%, or even from 3wt% to 10wt% sulphamic acid and/or water-soluble salts thereof.
- the sulphamic acid typically has the formula: H 2 NSO 3 H
- the sulphamic acid can be in zwitterionic form when present in the detergent composition; sulphamic acid in zwitterionic form has the formula: H 3 N + SO 3 - Possibly at least part of, possibly all of, the sulphamic acid is in zwitterionic form when present in the composition, for example as a separate particulate component.
- the sulphamic acid can improve the dispensing and disintegration of the detergent composition. It is capable of reacting with a source of carbonate, if present, in an aqueous environment such as the wash liquor in the drum of an automatic washing machine or in the dispensing drawer of an automatic washing machine or some other dispensing device such as a ball (granulette) or a net, to produce carbon dioxide gas.
- a source of carbonate if present, in an aqueous environment such as the wash liquor in the drum of an automatic washing machine or in the dispensing drawer of an automatic washing machine or some other dispensing device such as a ball (granulette) or a net, to produce carbon dioxide gas.
- the combination of sulphamic acid and a source of carbonate is an effervescence system that can improve the dispensing performance of the detergent composition.
- the extra agitation in the wash liquor provided by this effervescence system can also improve the cleaning performance of the detergent composition.
- Sulphamic acid has a very low hygroscopicity, significantly lower than other acids such as citric acid, malic acid or succinic acid; sulphamic acid does not readily pick up water. Sulphamic acid is stable during storage of the detergent composition and does not readily degrade other components of the detergent composition under certain storage conditions such as high humidity. Surprisingly, the sulphamic acid is stable even in the presence of mobile liquid phases, for example non-ionic detersive surfactants. Even more surprisingly, the sulphamic acid does not readily degrade perfumes during storage under high humidity.
- the sulphamic acid, and/or water-soluble salts thereof is in particulate form.
- the sulphamic acid, and/or water-soluble salts thereof is preferably in particulate form and preferably is incorporated into the detergent composition in the form of dry-added particles, preferably in the form of separate dry-added particles.
- the sulphamic acid may be in the form of a co-particulate admixture with a source of carbonate, this co-particulate admixture may be produced by methods such as agglomeration (including pressure agglomeration), roller compaction, extrudation, spheronisation, or any combination thereof.
- agglomeration including pressure agglomeration
- roller compaction roller compaction
- extrudation spheronisation
- the sulphamic acid, and/or water-soluble salts thereof, in particulate form has a weight average particle size in the range of from 210 micrometers to 1,200 micrometers, or preferably from 250 micrometers to 800 micrometers.
- the sulphamic acid, and/or water-soluble salts thereof, in particulate form has a particle size distribution such that no more than 35wt% of the sulphamic acid, and/or water-soluble salts thereof, has a particle size of less than 250 micrometers, preferably no more than 30wt% of the sulphamic acid, and/or water-soluble salts thereof, has a particle size of less than 250 micrometers, and preferably no more than 35wt% of the sulphamic acid, and/or water-soluble salts thereof, has a particle size of greater than 1,000 micrometers, preferably no more than 25wt% of the sulphamic acid, and/or water-soluble salts thereof, has a particle size of greater than 1,000 micrometers.
- Sulphamic acid, and/or water-soluble salts thereof has a superior building capability than other acids such as citric acid, malic acid, succinic acid and salts thereof.
- Sulphamate which is either incorporated in the composition or is formed in-situ in the wash liquor by the in-situ neutralisation of sulphamic acid, has a high binding efficiency with free cations (for example, such as calcium and/or magnesium cations to form calcium sulphamate and/or magnesium sulphamate, respectively).
- This superior building performance due to the presence of sulphamic acid, and/or water-soluble salts thereof, in the detergent composition is especially beneficial when the detergent composition comprises very low levels of, or no, zeolite builders and phosphate builders, when cleaning negatives associated with a high concentration of free calcium and/or magnesium are most likely to occur.
- composition may comprise at least 1 wt%, or at least 2wt%, or at least 3wt%, or at least 4wt%, or even at least 5wt% polymeric polycarboxylates.
- High levels of polymeric polycarboxylate can act as builders and sequester free calcium ions in the wash liquor, they can also act as soil dispersants and can provide an improved particulate stain removal cleaning benefit.
- Preferred polymeric polycarboxylates include: polyacrylates, preferably having a weight average molecular weight of from 1,000Da to 20,000Da; co-polymers of maleic acid and acrylic acid, preferably having a molar ratio of maleic acid monomers to acrylic acid monomers of from 1:1 to 1:10 and a weight average molecular weight of from 10,000Da to 200,000Da, or preferably having a molar ratio of maleic acid monomers to acrylic acid monomers of from 0.3:1 1 to 3:1 and a weight average molecular weight of from 1,000Da to 50,000Da.
- the composition comprises at least 1wt%, or at least 2wt%, or at least 3wt% soil dispersants.
- the composition typically comprises adjunct components.
- adjunct components include: bleach such as percarbonate and/or perborate, preferably in combination with a bleach activator such as tetraacetyl ethylene diamine, oxybenzene sulphonate bleach activators such as nonanoyl oxybenzene sulphonate, caprolactam bleach activators, imide bleach activators such as N-nonanoyl-N-methyl acetamide, preformed peracids such as N,N-pthaloylamino peroxycaproic acid, nonylamido peroxyadipic acid or dibenzoyl peroxide; chelants such as diethylene triamine pentaacetate, diethylene triamine penta(methyl phosphonic acid), ethylene diamine-N'N'-disuccinic acid, ethylene diamine tetraacetate, ethylene diamine tetra(methylene phosphonic acid) and hydroxyethane di(methylene phosphonic acid); enzymes such as am
- the composition comprises less than 1wt% chlorine bleach and less than 1wt% bromine bleach.
- the composition is essentially free from bromine bleach and chlorine bleach. By “essentially free from” it is typically meant “comprises no deliberately added”.
- the composition is for use for laundering delicate fabrics, then preferably the composition is essentially free from bleach, and/or essentially free from protease and/or from 0wt% to less than 0.1wt% fluorescent whitening components.
- essentially free from it is typically meant “comprises no deliberately added”. This is preferred when it is desirable to provide a good fabric care when laundering delicate fabrics such as silk and/or wool.
- the composition may also preferably comprise from 0wt% to less than 20wt% sodium citrate, or from 0wt% to 10wt%, or from 0wt% to 5wt%, or from 0wt% to 1wt% sodium citrate.
- the composition may also preferably comprise from 0wt% to 2wt% trisodium sulphosuccinate, or from 0wt% to 1wt%, or from 0wt% to 0.1wt% trisodium sulphosuccinate. This is preferred in order to optimise the space in the formulation.
- the composition can be in any solid form such as an agglomerate, a spray-dried power, an extrudate, a flake, a needle, a noodle, a bead, or any combination thereof.
- the detergent composition is in the form of free-flowing particles.
- free-flowing particles it is typically meant that the composition is in the form of separate discrete particles.
- the detergent composition in free-flowing particulate form typically has a bulk density of from 450g/l to 1000g/l, preferred low bulk density detergent compositions have a bulk density of from 550g/l to 650g/l and preferred high bulk density detergent compositions have a bulk density of from 750g/l to 900g/l.
- the composition is typically contacted with water to give a wash liquor having a pH of from above 7 to less than 13, preferably from above 7 to less than 10.5. This is the optimal pH to provide good cleaning whilst also ensuring a good fabric care profile.
- composition may be made by any suitable method including agglomeration, spray-drying, extrusion, mixing, dry-mixing, liquid spray-on, roller compaction, spheronisation or any combination thereof.
- the composition upon contact with water at a concentration of 9.2g/l and at a temperature of 20°C forms a transparent wash liquor having (i) a turbidity of less than 500 nephelometric turbidity units; and (ii) a pH in the range of from 8 to 12.
- the resultant wash liquor has a turbidity of less than 400, or less than 300, or from 10 to 300 nephelometric turbidity units.
- the turbidity of the wash liquor is typically measured using a H1 93703 microprocessor turbidity meter.
- a typical method for measuring the turbidity of the wash liquor is as follows: 9.2g of composition is added to 1 litre of water in a beaker to form a solution. The solution is stirred for 5 minutes at 600rpm at 20°C. The turbidity of the solution is then measured using a H1 93703 microprocessor turbidity meter following the manufacturer's instructions.
- the composition typically has an equilibrium relative humidity of from 0% to less than 30%, preferably from 0% to 20%, when measured at a temperature of 35°C.
- the equilibrium relative humidity is determined as follows:
- 300g of composition is placed in a I litre container made of a water-impermeable material and fitted with a lid capable of sealing the container.
- the lid is provided with a sealable hole adapted to allow insertion of a probe into the interior of the container.
- the container and its contents are maintained at a temperature of 35°C for 24 hours to allow temperature equilibration.
- a solid state hygrometer (Hygrotest 6100 sold by Testoterm Ltd, Hapshire, UK) is used to measure the water vapour pressure. This is done by inserting the probe into the interior of the container via the sealable hole in the container's lid and measuring the water vapour pressure of the head space. These measurements are made at 10 minute intervals until the water vapour pressure has equilibrated. The probe then automatically converts the water vapour pressure reading into an equilibrium relative humidity value.
- the detergent product comprises a combination of a composition and a packaging system.
- the composition is defined in more detail above.
- the packaging system is defined in more detail below.
- the packaging system has a moisture vapour transfer rate of from 0gm -2 day -1 , preferably less than 10gm -2 day -1 .
- the moisture vapour transfer rate is typically measured by any suitable method known in the art, preferred methods include ASTM Standard E-96-53T or TAPPI Standard T464 m-45.
- the preferred method is ASTM Standard E-96-53T.
- the packaging system may be in the form of a box, bag, bottle, tin, can, packet, sachet, drum.
- the packaging system is in the form of a bottle.
- the bottle is translucent. The stability of the composition is improved when it is stored in a packaging system having a very low vapour transfer rate.
- Example 1 A particulate laundry detergent composition and process of making it.
- Aqueous slurry composition Aqueous slurry composition.
- An aqueous slurry having the composition as described above is prepared having a moisture content of 25.89%.
- the aqueous slurry is heated to 72°C and pumped under high pressure (from 5.5x10 6 Nm -2 to 6.0x10 6 Nm -2 ), into a counter current spray-drying tower with an air inlet temperature of from 270°C to 300°C.
- the aqueous slurry is atomised and the atomised slurry is dried to produce a solid mixture, which is then cooled and sieved to remove oversize material (>1.8mm) to form a spray-dried powder, which is free-flowing.
- Fine material ( ⁇ 0.15mm) is elutriated with the exhaust the exhaust air in the spray-drying tower and collected in a post tower containment system.
- the spray-dried powder has a moisture content of 1.0wt%, a bulk density of 427g/l and a particle size distribution such that 95.2wt% of the spray-dried powder has a particle size of from 150 to 710 micrometers.
- the composition of the spray-dried powder is given below.
- the anionic detersive surfactant particle 1 is made on a 520g batch basis using a Tilt-A-Pin then Tilt-A-Plow mixer (both made by Processall). 108g sodium sulphate supplied is added to the Tilt-A-Pin mixer along with 244g sodium carbonate. 168g of 70% active C 25 E 3 S paste (sodium ethoxy sulphate based on C 12/15 alcohol and ethylene oxide) is added to the Tilt-A-Pin mixer. The components are then mixed at 1200rpm for 10 seconds. The resulting powder is then transferred into a Tilt-A-Plow mixer and mixed at 200rpm for 2 minutes to form particles.
- the particles are then dried in a fluid bed dryer at a rate of 25001/min at 120°C until the equilibrium relative humidity of the particles is less than 15%.
- the dried particles are then sieved and the fraction through 1180 ⁇ m and on 250 ⁇ m is retained.
- the composition of the anionic detersive surfactant particle 1 is as follows:
- the cationic surfactant particle 1 is made on a 14.6kg batch basis on a Morton FM-50 Loedige mixer. 4.5kg of micronised sodium sulphate and 4.5kg micronised sodium carbonate are premixed in the Morton FM-50 Loedige mixer. 4.6kg of 40% active mono-C 12-14 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride (cationic surfactant) aqueous solution is added to the Morton FM-50 Loedige mixer whilst both the main drive and the chopper are operating. After approximately two minutes of mixing, a 1.0kg 1:1 1 weight ratio mix of micronised sodium sulphate and micronised sodium carbonate is added to the mixer.
- the resulting agglomerate is collected and dried using a fluid bed dryer on a basis of 25001/min air at 100-140°C for 30 minutes.
- the resulting powder is sieved and the fraction through 1400 ⁇ m is collected as the cationic surfactant particle 1.
- the composition of the cationic surfactant particle 1 is as follows:
- 10.84kg of the spray-dried powder of example 1, 4.76kg of the anionic detersive surfactant particle 1, 1.57kg of the cationic detersive surfactant particle 1 and 7.83kg (total amount) of other individually dosed dry-added material are dosed into a I m diameter concrete batch mixer operating at 24rpm. Once all of the materials are dosed into the mixer, the mixture is mixed for 5 minutes to form a granular laundry detergent composition.
- the formulation of the granular laundry detergent composition is described below: Sodium percarbonate (having from 12% to 15% active AvOx) 14.70 Photobleach particle 0.01 Lipase (11.00mg active/g) 0.70 Amylase (21.55mg active/g) 0.33 Protease (56.00mag active/g) 0.43 Tetraacetyl ethylene diamine agglomerate (92wt% active) 4.35 Suds suppressor agglomerate (11.5wit% active) 0.87 Acrylat/maleae copolymer particle (95.7wt% active) 0.29 Green/Blue carbonate speckle 0.50 Anionic detersive surfactant particle 1 19.04 Cationic detersive surfactant particle 1 6.27 Sodium sulphate 3.32 Solid perfume particle 0.63 Total Parts 100.00
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US60046404P | 2004-08-11 | 2004-08-11 | |
PCT/US2005/028587 WO2006020789A1 (en) | 2004-08-11 | 2005-08-11 | A highly water-soluble solid laundry detergent composition that forms a clear wash liquor upon dissolution in water |
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EP1776442A1 EP1776442A1 (en) | 2007-04-25 |
EP1776442B1 true EP1776442B1 (en) | 2010-05-26 |
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EP05786488A Active EP1776442B1 (en) | 2004-08-11 | 2005-08-11 | A highly water-soluble solid laundry detergent composition that forms a clear wash liquor upon dissolution in water |
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US (1) | US7605116B2 (zh) |
EP (1) | EP1776442B1 (zh) |
JP (1) | JP4932713B2 (zh) |
KR (1) | KR20070036170A (zh) |
CN (1) | CN101001941B (zh) |
AR (1) | AR050127A1 (zh) |
AT (1) | ATE469202T1 (zh) |
AU (1) | AU2005272745A1 (zh) |
BR (1) | BRPI0514300A (zh) |
CA (1) | CA2573996C (zh) |
DE (1) | DE602005021502D1 (zh) |
EG (1) | EG24802A (zh) |
ES (1) | ES2346671T3 (zh) |
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WO (1) | WO2006020789A1 (zh) |
Families Citing this family (51)
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EP1693438A1 (en) * | 2005-02-21 | 2006-08-23 | The Procter & Gamble Company | A particulate laundry detergent composition comprising a detersive surfactant, carbonate and a cellulosic polymer |
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CN109790490A (zh) * | 2016-10-03 | 2019-05-21 | 宝洁公司 | 衣物洗涤剂组合物 |
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AU477001B2 (en) * | 1972-11-13 | 1976-10-14 | The Procter & Gamble Company | Detergent compositions |
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US5663136A (en) | 1992-06-15 | 1997-09-02 | The Procter & Gamble Company | Process for making compact detergent compositions |
ATE169667T1 (de) | 1993-07-14 | 1998-08-15 | Procter & Gamble | Reinigungsmittel-verpackung-kombination |
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DE69923196T2 (de) * | 1998-09-25 | 2005-12-29 | The Procter & Gamble Company, Cincinnati | Waschmittelgranulate |
CN1322242A (zh) * | 1998-09-25 | 2001-11-14 | 宝洁公司 | 洗涤剂组合物 |
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GB2343456A (en) * | 1998-11-06 | 2000-05-10 | Procter & Gamble | Speckle particles and compositions containing the speckle particles |
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GB2344597A (en) * | 1998-12-08 | 2000-06-14 | Procter & Gamble | Effervescence components |
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US6939841B2 (en) * | 2002-11-21 | 2005-09-06 | S.C. Johnson & Son, Inc. | Effervescent compositions |
-
2005
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- 2005-08-11 BR BRPI0514300-4A patent/BRPI0514300A/pt not_active Application Discontinuation
- 2005-08-11 CA CA2573996A patent/CA2573996C/en not_active Expired - Fee Related
- 2005-08-11 MX MX2007001670A patent/MX2007001670A/es active IP Right Grant
- 2005-08-11 JP JP2007525797A patent/JP4932713B2/ja active Active
- 2005-08-11 EP EP05786488A patent/EP1776442B1/en active Active
- 2005-08-11 KR KR1020077003221A patent/KR20070036170A/ko not_active Application Discontinuation
- 2005-08-11 ES ES05786488T patent/ES2346671T3/es active Active
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- 2005-08-11 AR ARP050103364A patent/AR050127A1/es not_active Application Discontinuation
- 2005-08-11 CN CN2005800273421A patent/CN101001941B/zh active Active
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CA2573996A1 (en) | 2006-02-23 |
MX2007001670A (es) | 2007-04-10 |
EG24802A (en) | 2010-09-15 |
EP1776442A1 (en) | 2007-04-25 |
AR050127A1 (es) | 2006-09-27 |
CN101001941A (zh) | 2007-07-18 |
WO2006020789A1 (en) | 2006-02-23 |
US20060035802A1 (en) | 2006-02-16 |
CN101001941B (zh) | 2012-03-21 |
BRPI0514300A (pt) | 2008-06-10 |
ATE469202T1 (de) | 2010-06-15 |
ES2346671T3 (es) | 2010-10-19 |
KR20070036170A (ko) | 2007-04-02 |
AU2005272745A1 (en) | 2006-02-23 |
DE602005021502D1 (de) | 2010-07-08 |
JP2008509278A (ja) | 2008-03-27 |
JP4932713B2 (ja) | 2012-05-16 |
CA2573996C (en) | 2010-09-21 |
US7605116B2 (en) | 2009-10-20 |
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